In this instalment of "Sample Preparation Perspectives," Norwegian authors from the University of Oslo describe the practical aspects of hollow fibre liquid-phase microextraction in the three-phase mode (HF3LPME). The guest authors highlight important practical issues related to the supported liquid membrane, the hollow fibre and the extraction itself. They also discuss practical work with electromembrane extraction (EME), which is related to HF3LPME but uses an electrical potential as the driving force for the extraction.

This month's instalment describes practical aspects of hollow-fibre liquidphase microextraction in the three-phase mode (HF3LPME). HF3 LPME is a microscale sample preparation technique (1) where target analytes are extracted from an aqueous sample through a supported liquid membrane (SLM) that is immobilized in the pores of a porous polymeric material and into a volume of acceptor solution (typically, 10–30 µL). In this context, the porous polymeric material is a hollow fibre. Here, we highlight important practical issues related to the SLM, the hollow fibre and the extraction itself because these issues are important for successful HF3LPME. We also discuss practical work with electromembrane extraction (EME), which is related to the HF3LPME device but uses an electrical potential as the driving force for the extraction (2).

HF3LPME can be used for extraction of basic or acidic analytes from aqueous samples. Figure 1 illustrates a setup for HF3LPME. The sample is contained in a sample vial and the pH is adjusted in the sample before extraction to keep the analytes in their uncharged state. For basic analytes, the sample is made alkaline, and for acidic analytes, the sample is acidified. A small piece of a porous hollow fibre, typically made of polypropylene, is closed in one end and dipped in an organic solvent immiscible with water. In a few seconds, this organic solvent is immobilized in the pores in the wall of the hollow fibre by capillary forces, forming an SLM.

A 10–30 µL volume of aqueous acceptor solution is then injected into the lumen of the hollow fibre. For basic analytes, the acceptor solution is acidic, whereas it is alkaline for acidic analytes. The hollow fibre is finally placed into the sample and the whole assembly (sample vial and hollow fibre) is agitated for typically 15–45 min. During this time, analyte molecules are extracted in their uncharged state from the sample into the SLM, and further into the acceptor solution. In the acceptor solution, the analyte molecules become ionized, which prevents them from re-entering the SLM. After extraction, the acceptor solution is collected and analysed directly by high performance liquid chromatography (HPLC), capillary electrophoresis (CE), mass spectrometry (MS) or other related analytical techniques.

The major advantages of HF3LPME can be summarized as follows:

High enrichment (up to 25,000-fold) (3)

Excellent sample clean-up

Direct compatibility with HPLC, CE and MS

Low solvent consumption (10–30 µL of solvent for each extraction).

Advantages, as well as limitations, of HF3LPME have been discussed substantially in the literature and several reviews discussed a broad range of applications (4–11).

Author Guidelines

LCGC welcomes manuscripts that describe techniques and applications of all forms of chromatography and capillary electrophoresis and that are of immediate interest to users in industry, academia, and government. For more info, see our full page of author guidelines.